Compounds with symmetrical tricobalt chains wrapped by dipyridylamide ligands and cyanide or isothiocyanate ions as terminal ligands

Three new linear compounds of the type Co(3)(dpa)(4)X(2), where dpa is the anion of di(2-pyridyl)amine and X is NCS(-) (5), CN(-) (6), and N(CN)(2)(-) (7), have been prepared, and their structures and magnetic behavior have been studied. In all of them, including three different solvates of 5, the Co(3) chains are symmetrical with Co-Co distances of ca. 2.31-2.32 A. The appearance of four lines in the (1)H NMR spectra of the three compounds is also consistent with a symmetrical structure in solution. For all compounds, the magnetic behavior is quite similar with mu(eff) of ca. 1.9-2.0 micro(B) at temperatures between 1.8 and 200 K. As the temperature increases, the effective moments increase gradually, but since saturation is not reached, even at 400 K, the high-spin state cannot be assigned.     

Synthesis and Structural Characterization of cis- and trans-bis(4,4′-dimethyl-2,2′-bipyridine)cadmium(II) Nitrates Prepared in a One-pot Reaction

The cis and trans isomers of [Cd(dmbpy)₂](NO₃)₂] (dmbpy = 4,4′-dimethyl-2,2′-bipyridine) have been synthesized simultaneously via a one-pot reaction of Cd(NO₃)₂ · 4H₂O with the dmbpy ligand in a MeOH/H₂O mixture; they can be obtained individually by means of the mechanical separation due to their different growing habit of the single-crystals. Different π-stacking interactions are observed in the cis and trans isomers forming different one-dimensional networks. The outcome of the DFT calculations agrees well with the experimental results.     

Determination of dispersity of crushed granite

Summary Experimental crushed granite column breakthrough curves, using ⁹⁹Tc as spike tracer and ³H as invariant tracer, were analyzed by different linear regression techniques. Dispersity of crushed granite and the retardation factor of ⁹⁹TcO₄^- on the crushed granite were determined simultaneously by one linear regression. Dispersity of crushed granite was also obtained with ³H as invariant tracer by the other linear regression. The dispersities found by spike source and invariant source methods are compared. Experimental results show that the dispersity found by the spike source method is close to that found by the invariant source method. This indicates that dispersity is only a characteristic of the dispersion medium.     

Ion flotation of rhodium(III) and palladium(II) with anionic surfactants

The ion flotation of rhodium(III) and palladium(II) with some anionic surfactants has been investigated. Two flotation procedures are proposed for the separation of some platinum metals, based on differences in the kinetic properties of the chloro-complexes of rhodium(III), palladium(II) and platinum(IV). The first involves the selective flotation of Rh(H(2)O)(3+)(6) from PdCl(2-)(4) and PtCl(2-)(6) in dilute hydrochloric acid with sodium dodecylbenzenesulfonate (SDBS). After precipitation of the hydroxide and redissolution in dilute acid, the Rh(III) is converted into Rh(H(2)O)(3+)(6), Pd(II) and Pt(IV) remaining as PdCl(2-)(4) and PtCl(2-)(6) respectively, and separation is achieved by floating the Rh(H(2)O)(3+)(6) with SDBS. The second is for separation of Pd(II). Prior to flotation, the solution of PdCl(2-)(4) and PtCl(2-)(6) is heated with ammonium acetate to convert PdCl(2-)(4) into Pd(NH(3))(2+)(4). The chloro-complex of Pt(IV) is unaffected. The complex cation, Pd(NH(3))(2+)(4), is then selectively floated with SDBS. The procedures are fast, simple and do not require expensive reagents and apparatus.     

PA.FPNS: its synthesis and use in spectrophotometric determination of magnesium

A new polymeric chromogenic reagent PA.FPNS has been synthesized by condensing polyallylamine (PA) with 3-(4-formylphenylazo)-4,5-dihydroxynaphthalene-2,7-disulfonic acid (FPNS) and its properties studied. In alkaline media, PA.FPNS reacts with magnesium to form a water-soluble blue complex, whose absorption maximum is at 604 nm. The molar absorptivity (varepsilon) of the complex is 5.2 x 10(4)l mol(-1) cm(-1), which is four times that of the FPNS-Mg complex, and Beer's law is obeyed over the range 0-0.35 mug ml(-1) magnesium. Compared to the corresponding low-molecular-weight FPNS and other chromogenic reagents, PA.FPNS offers considerably improved sensitivity and selectivity for magnesium, which may be attributed to incorporating FPNS into a water-soluble polymer and the effect of the polymeric chain on the reaction microenvironment. Also, a simple and sensitive spectrophotometric method for the determination of magnesium has been developed and applied to water and human fluid samples with satisfactory results.     

Crystalline titanium dichloride—an active catalyst in ethylene polymerization. II. Polymer structure,polymerization variables,and scope

Polymerization of ethylene with ball-milled titanium dichloride leads to a completely linear polymer with terminal unsaturation corresponding to approximately one carbon–carbon double bond per molecule. Polymerization rate is first-order in both monomer and catalyst concentration at 140°C. Due to a thermal deactivation of the catalyst, the polymerization rate falls sharply with temperature above 180°C. Propylene and butene-1 will copolymerization with ethylene in this system, propylene more efficiently than butene-1. Evidence for copolymerization of trans-2-butene, but not of the cis-isomer or of isobutene, in trace concentrations is presented. Propylene is homopolymerized to a product low in isotactic content. The significance of the structural and (limited) kinetic data in terms of the mechanism of polymerization are discussed.     

Immunosuppressive ent‐Kaurene Diterpenoids from Isodon serra

Three new enmein‐type ent‐kaurenoids, i.e., the two pairs 1 and 2 of 20‐epimers and the (20R)‐isomer 3 , besides the seven known diterpenoids 4 – 10 , were isolated from the aerial parts of Isodon serra. Their structures were elucidated by spectroscopic techniques and X‐ray diffraction. The immunosuppressive effect for T‐lymphocytes proliferation induced by Con A in BALB/c mouse was evaluated for the isolates 1 – 10 . They all displayed a remarkable inhibitory effect, with multi‐glycosides of Tripterygium wilfordii as positive reference substance (Table 3).     

Virus Particles Monitored by Fluorescence Spectroscopy: A Potential Detection Assay for Macromolecular Assembly¶

Native fluorescence spectroscopy was used for in situ investigations of two lipid‐containing bacteriophages from the cystovirus family as well as their Pseudomonad host cells. Both the viruses φ6 and φ12 and their bacterial host proteins contain the amino acid tryptophan (trp), which is the predominant fluorophore in UV. Within proteins, trp's structural environment differs, and the differences are reflected in their spectroscopic signatures. It was observed that the peak of the trp emission from both viruses was at 330 nm, a significantly shorter wavelength than trp in either the Pseudomonad host cells or the amino acid's chemical form. This allowed us to monitor the viral attachment process and subsequent lytic release of progeny virus particles by measurement of the trp emission spectra during the infection process. This work demonstrates that fluorescence may offer a novel tool to detect viruses and monitor viral infection of cells and may be part of a biodefense application.     

Instrumental neutron activation analysis of large samples: A pilot experiment

A large sample INAA (LS-INAA) was conducted based on available experimental conditions. Four different materials, e.g., a quartz-sand and three wastes from an incineration plant were analyzed on sample size of 1 kg. The neutron flux spatial distribution was determined by irradiation of flux monitors in the sample. The gamma-ray apparent counting efficiency was evaluated based on the effective-solid angle concept, using linear attenuation coefficients calculated from an iteration process. The k ₀- and the modified monostandard methods were modified for the LS-INAA. To check the LS-INAA performance, a conventional small sample INAA was carried out for the quartz sand and a waste. All detected elements in the LS-INAA are presented and the discussion is conducted to explore the sources of errors in the LS-INAA. As a pilot experiment, the information from this work will be used in constructing irradiation and counting devices for the new FRM-II neutron source in Garching, Germany.